Document 5LLOEdvx0beeERgDze1yJro6N
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CONFIDENTIAL
Attached Is the Reactor Opening Loss (ROL) data completed as of August 5, 1985 using the hot box sampling method. A total of 146 sample8 was taken, 129 of these were valid samples, and 17 were invalid samples due to problems with the sampling system equipment. A complete report with portable hydrocarbon detector data will be Issued by Process Engineering Department at a later
date.
The attached summary sheet divides the samples into the following categories: stripping procedure used, number of valid and invalid samples, use of reactor and condenser sample tubes, and the number of valid samples above ROL limits. Stripping procedures are described in the Appendix and labeled by letters A through I. Stripping Procedure A is the current stripping procedure used at the plant. The stripping procedures are less severe than Procedure A and were used to determine how sensitive ROL data is to stripping conditions. Log sheets a&d batch sheets for all samples taken are Included in the Appendix.
When it was realized that polymer buildup inside reactor and condenser nozzles could affect sample results, sample tubes inserted into the reactor headspace where possible to ensure a clean sampling path. A sample tube was also Inserted into the condenser of reactor 700 after pluggage problems and polymer buildup was found in the condenser's sampling nozzle. Also, after problems with steam tracing on the sample lines and hot boxes were encountered, steam tracing was verified to be above 300F before samples were taken.
Problems with sampling equipment invalidated certain samples. Problems due to sample line pluggage and polymer buildup Inside reactor and condenser sample nozzles invalidated samples on the following reactor batches:
Date
Reactor
Batch No.
Blend No
1. 4/2/85 2. 4/3/85 3. 4/4/85 4. 4/4/85 5. 4/16/85 6. 4/16/85 7. 4/17/85 8. 4/22/85 9. 4/23/85 10.4/23/85 11.6/21/85 12.6/22/85 13.7/8/85 14.7/9/85
744 300 743 743 743 744 600 700 700 700 700 700 700 700
492 3615 1015 1016 1051
538 5205 2713 2715 2716 2830 2833 2858 2859
38991 60243 39024 39030 39211 39214 60447 60529 60539 60544 61275 61296 61414 61424
A
VAB.0001102762
4
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CONFIDENTIAL
Problems with stea tracing on sample lines where steam tracing was not hot enough or completely shut off, invalidated the following samples:
Date
Reactor
Batch No*
Blend No
15. 6/3/85 16. 6/3/85
400 600
5419 5327
61053 61052
Problems with air leakage into the sampling system invalidated the following sample:
Date
Reactor
Batch No.
Blend No
17.4/15/85
300
3651
60425
Invalid samples no. 1,6,7,8,9,11,12,13, and 14 were caused by verified polymer buildup and pluggage in the reactor/condenser sample nozzles on sample lines. In each case, the actual pluggage in the line was discovered and either drilled out or removed. Evidence that the lines were plugged was usually indicated by a difference in the reactor and condenser sample line pressures when pulling sample vapors. Whenever these lines showed a pressure difference of more than 2" Hg, pluggage was suspected and usually sampling was aborted. Sometimes the sample line pressures would fluctuate as sample was being pulled from the reactor/condenser, indicating polymer chunks inside the sample line. Experience has indicated that sample lines that contain a buildup of polymer give erroneous results when the samples are analysed due to residual vinyl chloride monomer in the polymer.
Invalid samples no. 2,3,4,5,and 10 were caused by sample line pluggage also. This was indicated by the difference in the reactor and condenser line pressures while sample vapors were being pulled from the reactor/condenser. This was usually double-checked after the reactor was dumped. When pulling sample from a reactor/condenser at atmospheric pressure, a clear line would give a reading of no more than 4" to 5" Hg on the sample line vacuum gauge. Any reading higher than this Indicated pluggage and corrective action had to be taken. In some instances, the pluggage would dissappear when vacuum on the reactor/condenser was broken to dump the reactor, thus no verified evidence that polymer was in the sample line was obtainable. Any line pressure differences exceeding 2" Hg indicated pluggage in the line.
Invalid samples no. 15 and 16 were caused by the fact that the samples were taken, the steam tracing on one of the sample lines was not on. The steam traced sample lines must be hot enough to keep sample vapors from condensing while being pulled through the sample line. Otherwise, water vapor will condense and the percent vinyl chloride monomer in the sample vapor will
After problems with the steam tracing were discovered, all steam tracing temperatures were checked before a sample was taken.
VAB.0001102763
CONFIDENTIAL
Invalid sample no. 17 had a leak on the reactor sample line. All sample lines and bombs were vacuum checked before a sample was taken. This leak wad discovered after the sample was taken and was traced to a leaking pressure gauge connection.
The conversion factors used in calculating the amount of slurry produced were based on the Aberdeen Resin Economics Program Issued August 6, 1984 by Process Engineering Department.
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The volume used to make the ROL calculation was measured on 5385 resin and 5465 resin. Volumes for the other products were calculated using the measured volumes as a basis.
The sample bomb temperature correction factors, as described in the ROL Sample Calculation section of this report, were calculated using sample bomb surface temperatures. These temperature measurements were made with a hand-held surface temperature thermocouple probe. This procedure required that the hot box be opened after the actual sample was taken. This delay, and opening the box, resulted in some sample bomb surface temperatures that were below reactor or condenser operating temperatures at the time of sampling. Whenever this happened, no temperature correction factor was used.
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APPENDIX VAB.0001102772
PVC REACTOR STRIPPING PROCEDURE A
Products; 5265, 5305, 5385, 5425, 5465 - Both Modules
1. Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start injecting steam into the reactor (old module reactors only)
4. After the vacuum pumps have come on, bring the slurry temperature up to the following temperature and hold (slurry temperature some times overshoots set point).
5385, 5425, 5465 both modules - 215F 5305, 5265 both modules - 210F
5. When the slurry begins to boil, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the above set point without cooling until the reactor head space temperature has risen above the following limits for 10 minutes.
215F 210F
Reactor Head Space T
195F 190F
erature
Turn the full cooling water on the condenser and open the dump valve and recover the dump manifold.
7. After the cooling has been on five minutes, cut off steam and con tinue cooling.
8. When the slurry cools to 195F, turn off the cooling water.
9. Dump the reactor.
VAB.0001102773
PVC REACTOR STRIPPING PROCEDURE B
COffIDENTIAL
Products: 5385 - Old M ' " ~ "
1. Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start Injecting steam Into the reactor.
4. After the vacuum pumps have come on, bring the slurry temperature up to 205 F and hold (slurry temperature sometimes overshoots set point).
5. When the slurry begins to boll, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the above set point without cooling until the reactor head space temperature has risen to the following limits:
205F
Reactor He *
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200F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When Che slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
VAB.0001102774
PVC REACTOR STRIPPING PROCEDURE C
1;
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151
11
Products: 5385 - Old Module Only
1. Kill the reactor at the conditions prescribed on the product formula sheet
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start injecting steam into the reactor.
4. After the vacuum pumps have come on, bring the slurry temperature up to 200 F and hold (slurry temperature sometimes overshoots set point).
5. When the slurry begins to boil, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the above set point without cooling until the reactor head space temperature has risen to the following limits:
Slurry Temperature
/
Reactor Head Space Temperature
200F
195F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
A
VAB.0001102775
PVC REACTOR STRIPPING PROCEDURE D
Mi
Products: 5385,5305,5265 - Both Modules
1. Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start injecting steam into the reactor.
4. After the vacuum pumps have come on, bring the slurry temperature up to 195 F and hold (slurry temperature sometimes overshoots set point)
5. When the slurry begins to boll, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the above set point without cooling until the reactor head space temperature has risen to the following limits:
Slurry Temperature 195F
Reactor Head Space Temperature 190F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195 F, turn off the cooling water.
8. Dump the reactor.
A
VAB.0001102776
CONFIDENTIAL k
PVC REACTOR STRIPPING PROCEDURE E
Products: 5385 - Old Module Only
1. Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start Injecting steam into the reactor.
4. After the vacuum pumps come on, bring the slurry temperature up to 200F and hold (slurry temperature sometimes overshoots set point).
5. When the slurry begins to boll, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the above set point without cooling until the reactor head space temperature has risen to the following limits:
Slurry Temperature
Reactor H ' "
195F
195F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
VAB.0001102777
WI0ENTI4L
PVC REACTOR STRIPPING PROCEDURE F
Products; 5385 - Old Module Only
1. Rill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start Injecting steam into the reactor.
After the vacuum pumps have come on, bring the slurry temperature up to 205F and hold (slurry temperature sometimes overshoots set point).
5. When the slurry begins to boll, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the bove set point without cooling until the reactor head space temperature has risen to the following limits:
Slurry Temperature
Reactor Head Space Temperature
205F
200F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
PVC REACTOR STRIPPING PROCEDURE G
Products: 5385 - Old Module Only
1. Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start Injecting steam into the reactor.
4. After the vacuum pumps come on, bring the slurry temperature up to 210F and hold (slurry temperature sometimes overshoots set point).
5. When the slurry begins to boil, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the above set point without cooling until the reactor head space temperature has risen to the following limits:
Reactor Head Space Temperature
210F
205 F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
PVC REACTOR STRIPPING PROCEDURE H
Products; 5385 - Old Module Only
1* Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start injecting steam into the reactor.
4. After the vacuum pumps have come on, bring the slurry temperature up to 200F and hold (slurry temperature sometimes overshoot8 set point)
5. When the slurry begins to boll, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the bove set point without cooling until the reactor head space temperature has risen to the following limits for 5 minutes.
Slurry Temperature
Reactor Head Space Temperature
200F
195F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
i
VAB.0001102780
PVC REACTOR STRIPPING PROCEDURE I
CONFIDENM
Products: 5385 - Old Module Onl
1. Kill the reactor at the conditions prescribed on the product formula sheet.
2. Start the compressors and begin recovery.
3. Set the temperature set point at 180F and start Injecting steam Into the reactor.
4. After the vacuum pumps have come on, bring the slurry temperature up to 200F and hold (slurry temperature sometimes overshoots set point).
5. When the slurry begins to boll, the reactor head space temperature will rise rapidly and approach the slurry temperature. Hold the slurry temp at the bove set point without cooling until the reactor head space temperature has risen to the following limits for 10 minutes.
200 F
195F
6. Turn the full cooling water on the condenser, cut off steam, and open the dump valve and recover the dump manifold.
7. When the slurry cools to 195F, turn off the cooling water.
8. Dump the reactor.
SAMPLING PROCEDURE
J
The procedure used in sampling the reactor and condenser vapor space for ROL data is given below. Each step is listed in chronological order. Refer to the sampling system diagram in figure 1.
The same procedure was utilized throughout the sampling period except for the following two changes:
1. All samples were taken when the slurry temperature reached 195F on cool-down except for Procedure A samples prior to 5*29-85 (sample no. 77). Procedure A samples prior to 5-29-85 were taken when the slurry the temperature reached 200P on cool-down.
2. Beginning on 6/18/85 sample Insertion tubes were used to obtain reactor vapor space samples with the exception of sample no. 92. A sample insertion tube was also used on the condenser of reactor 700 beginning with sample no. 109. When the reactor pressure reached a vacuum, the half-inch stainless steel tubes were inserted into the vapor space. The tubes were long enough to clear the inside wall of the reactor/condenser by at least 6 inches. Once inserted, the tubes were secured with an air-tight connection and sample vapors could then be pulled from the reactor/condenser through the sampling system. The sample insertion tubes were used to ensure a clean, clear sample flow path.
In addition to these procedures, pertinent data was taken concerning each reactor batch sample and logged in on the sample logsheet (see appendix).
Procedure
1 Check that the steam tracing on the sample box and sampling line is turned on and that the bombs are installed Inside the box at least one hour prior to sampling. This will ensure that the system is hot when sampling begins. When the bombs are Installed, vacuum test the bombs and sampling lines for air leakage into the system by:
a. With the sampling box and bomb valves open (reactor valves closed) use the eductors to pull a vacuum on the system and note the pressure gauge reading on each side of the sampling box.
b. Close the bottom (eductor suction) valves on each side of the sample box.
c. Observe the pressure gauge reading on each side of the sampling box. If the pressure rises, there is a leak in the system which must be located and corrected before sampling.
d. Close the sample box valves and turn off eductors when finished.
After vacuum testing the system, leave the bomb valves open and close the sample box allowing the bombs to heatup.
VAB.0001102782
HP
Sampling Procedure Page 2 Procedure - continued
2. Begin pulling vapor out of the reactor/condenser through the sampling system five to ten minutes before the sample is to be taken. This is accomplished by turning on the eductors and opening the sample box and reactor sampling valves. Use a fresh air mask respirator to avoid VCM overexposure when in the vicinity of the sampling system while pulling vapor.
3. When the slurry is at the correct temperature* take the sample by: a. Close the bottom (eductor suction) valves on each side of the sample box. b. Wait three seconds for system pressure equalization. c. Close the top (sample line) valves on each side of the sample box.
/
d. Record the pressures shown on the sample pressure gauges on each side of the sample box.
e. Open the box and close the bomb valves. The above steps should be done in rapid succession. When completed* the reactor can be dumped. 4. Measure and record the surface temperature of each sample bomb. 5. Record which bomb and eductor were used for each sample. 6. Close the sample line valves on the reactor and condenser.
VAB.0001102783
FIGURE 1 - R.O.L. SAMPLING SYSTEM
srSM TPOCMD OAKO M&ad.*rmo C0/M)ma/sej
sreom taoc&O aod tOSULATSO AAACTWl SOHOLE A>WM
7b ATMOS aoucrao
mm SUOOLY
SO/ffPlE M0)t COVmWMfQ, SAMPLE S0MMS
TO Atmos EOucr&t
AMC snooty VAB.0001102784
ROL Sample Calculation
Attached Is a sample ROL calculation using data from D-600 reactor batch number 5207. The basis of the calculation Is also Included. A step-by-step description of the ROL calculation procedure follows.
After both reactor and condenser sample bombs were brought to the lab* they were allowed to cool to room temperature (24C) and then pressurized to 44.1 psia pressure using nitrogen. Next, the gas In the bombs was analyzed using a gas chromatograph. The results were measured In ppm on a volumetric basis (vppm) for the reactor and condenser bomb each.
At the 24C lab temperature and 44.1 psia pressure, the gas in the sample bombs was assumed ideal for calculation purposes. Utilizing the Ideal gas law, the total number of lb.-moles of gas in the bombs was calculated. This value, and the fact that vppm equals mole percent for an ideal gas, was used to calculate the lb .-moles of VCM in each of the reactor and condenser sample bombs.
The number of lb.--moles of VCM in each bomb was then corrected using a temperature correction factor. (The factors were calculated using bomb temperature data taken at the time of sampling.) The factor converts the number of lb.-moles of VCM in the 312 cu.cm, bomb to the number of lb.-moles of VCM in an equivalent 312 cu.cm, of reactor/condenser vapor space at sampling conditions.
The lb.-moles of VCM in 312 cu.cm, of reactor/condenser vapor space was next converted to lb. of VCM in each of the reactor and condenser vapor spaces by multiplying the number of lb.-moles of VCM in 312 cu.cm, of vapor space by the total vapor space volume and the molecular weight of VCM, and then dividing by the 312 cu.cm, volume
The total ROL was then calculated by dividing the number of pounds of VCM in the reactor and condenser vapor spaces by the millions of pounds of PVC produced, and then adding the results.
The slurry volumes used to obtain the reactor and condenser head space volumes were measured on 5385 and 5465 resin. Slurry volumes for the other products were calculated based on the measured volumes. All of the reactor head space volumes used in the ROL calculations include one-half of the condenser tube volume.
Conversion factors used in calculating the pounds of PVC produced were based on the Aberdeen Resin Economics Program issued August 6, 1984 by Process Engineering Department.
VAB.0001102785
TI
REACTOR OPENING LOSS SAMPLE CALCULATION
I. Basis of Calculation
1. Gas in bomb assumed to be ideal 2. 312 cu.cm* bomb volume (measured) 3. 24 C bomb temperature (average lab temperature) 4. Batch number 5207 sample data 5. 1.043 temperature correction factor for reactor bomb ppm 6. 1.006 temperature correction factor for condenser bomb ppm 7. 44.1 psia bomb pressure 8. 80.13% of factor used for conversion of 5385 resin.
II. Measure of VPFM of VCM in Bomb
Reactor bomb vppm * 289.2 vppm
Condenser bomb vppm * 4122 vppm
III. Calculate Lb.-Moles of Total Gas in Bomb
1 P 44.1 psia
2 V 312 cu.cm. 0.01102 cu.ft.
3 T 24C - 535.2R
4 R 10.73
5 n PV (44.1 psia)(0.01102 cu.ft.) 8.463 x 10 lb.-moles RT
IV. Calculate Lb.-Moles of VCM in Bomb by Ideal Gas Law
vppm * mole % (Ideal Gas Lav)
Ib.-moles VCM in reactor bomb " (289.2 x 10" ; -5 --8
(8.463 x 10 Lb.-moles total gas) * 2.448 x 10 lb.-moles VCM
Lb.-moles VCM in condenser bomb (4122 x 10~;
+
--5 -7 (8.463 x 10 lb.-moles total gas) 3.488 x 10 lb.-moles VCM
This is the lb.-moles of VCM in the bomb at 44.1 psia pressure which equals lb.-moles of VCM in the bomb when the sample is taken and the bomb valves are closed.
*
VAB.0001102786
Reactor Opening Loss Sample Calculation Page 2
V. Calculate Lb.-Moles of VCM in 312 cu.cm, of Reactor and Condenser Vapor Space
*
Temperature correction factor converts lb.-moles of VCM in 312 cu. cm. bomb volume to lb.-moles of VCM in 312 cu.cm, of reactor or condenser vapor space at the reactor/condenser temperature measured at time of sampling.
Lb.-moles VCM in 312 cu.cm, of reactor vapor space m
(2.448 x 10~8 lb.-moles VCM)(1.043) - 2.553 x 10-8 lb.-moles VCM
Lb.-Moles VCM in 312 cu.cm, of condenser vapor space * (3.488 x 10"7 lb.-moles VCM)(1.006) - 3.509 x 10"7 lb.-moles VCM
VI. Calculate Lb. of VCM in Reactor and Condenser Vapor Space
Total reactor vapor space 804.4 Total condenser vapor space 45.7 cu.ft.
I
312 cu.cm. * 0.01102 cu.ft.
VCM in reactor vapor space
g0
(804.4 cu.ft.)(2.553 x 10 lb.-moles VCM/0.01102 cu.ft.)
(62.5 lb.VCM/lb.-mole VCM) - 0.1165 lb. VCM
VCM in condenser vapor space (45.7 cu.ft.)(3.509 x 10"7 lb.-moles VCM/0.01102 cu.ft.)
(62.5 lb. VCM/lb.-mole VCM) - 0.0909 lb. VCM VII. Calculate Total ROL
Lb. PVC produced 0.03715 MM Lb. Reactor ROL 0.1165 lb. VCM/0.03715 MM lb. PVC -
3.14 lb. VCM/MM lb. PVC Condenser ROL * 0.0909 lb. VCM/0.03715 MM lb. PVC -
2.45 lb. VCM/MM lb. PVC Total ROL - 3.14 + 2.45 - 5.59 lb. VCM/MM lb. PVC
4
VAB.0001102787